CN104250582B - A kind of method that odorless white silkworm chrysalis oil is extracted in the leftover bits and pieces from silkworm chrysalis - Google Patents
A kind of method that odorless white silkworm chrysalis oil is extracted in the leftover bits and pieces from silkworm chrysalis Download PDFInfo
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Abstract
The invention discloses a kind of method that odorless white silkworm chrysalis oil is extracted in leftover bits and pieces from silkworm chrysalis, this method is after the drying of silkworm chrysalis leftover bits and pieces, crushing, thick silkworm chrysalis oil is extracted using ultrasonic wave added organic solvent, after modified graphene oxide progress adsorption treatment is added in the thick silkworm chrysalis oil of gained, filtering, obtains odorless white refined silkworm chrysalis oil；This method is simple to operate, quick, meets industrialized production, and obtained refined silkworm chrysalis oil is odorless, good decolorizing effect, and active ingredient has important application value without destruction.
Description
Technical field
The present invention relates to a kind of method that odorless white silkworm chrysalis oil is extracted in leftover bits and pieces from silkworm chrysalis, belongs to bio oil processing neck
Domain.
Background technology
Silkworm chrysalis is the principal by product of silk reeling industry, produce one ton of raw silk can one ton of dry pupa of by-product, its fat content is about
30%.Silkworm chrysalis oil is rich in a variety of unrighted acids needed by human of aliphatic acid particularly oleic acid, linoleic acid plus linolenic acid etc., tool
There is high nutritive value, oleic acid therein can be effectively reduced internal LDL (low density cholesterol), have prevention of arterial hard
The effect of change；Linoleic acid is also the important substance to sustain life, can change into gamma-Linolenic acid, DH- acid and gamma-linolenics and flower in vivo
Raw tetraenoic acid, then synthesis of prostaglandins can effectively treat angiocardiopathy, prevention myocardial infarction, and linoleic acid simultaneously can also be with
Cholesterol is esterified, and reduces internal serum, liver and blood cholesterol levels, the formation of atherosclerosis and arterial thrombus；α-
Leukotrienes can extend the metabolites such as synthesis eicosapentaenoic (EPA), 22 carbon six (DHA) through dehydrogenation and carbochain in vivo,
It is the life core substance for maintaining the evolution of mankind's brain, has and increase the multiple functions such as intelligence, protection eyesight, anti-aging, can
Effectively suppress thrombotic diseases, prevention myocardial infarction, cerebral infarction, reducing blood lipid, hypotensive, suppress hemorrhagic cerebral apoplexy, suppress
The generation and transfer of cancer, prevention and suppress senile dementia etc..
However, the silkworm chrysalis oil extracted from silkworm chrysalis is in crineous and has strong peculiar smell, if do not removed, directly as food
It is to be difficult to receive, even if as animal feed, can be also remained in animal meat, birds, beasts and eggs, limit its development and utilization.Mesh
Before the problem of there is no good method to remove silkworm chrysalis oil bad smell, this hampers application of the silkworm chrysalis oil in field of health care products significantly.
At present, the method for silkworm chrysalis oil deodorization decoloring mainly has following three kinds：H2O2Oxidizing process, organic solvent infusion process and work
Property carbon adsorption.H2O2Oxidizing process decolorizing effect is preferable, and H2O2There is heat resolve Cheng Shui advantage, but its amino acid is by tight
Destroy, queried in food using the security of its product again；Organic solvent infusion process can only remove oleophylic, lower boiling
Malodoring substance, deodorization decoloring effect are undesirable.Activated carbon to silkworm chrysalis oil deodorization decoloring effect compared with the prior art in other sides
Method is preferable, but activated carbon separates highly difficult from silkworm chrysalis oil, causes the subsequent treatment of decolouring and deodorizing extremely difficult, and adsorption loss
Rate is larger.
The content of the invention
For silkworm chrysalis oil of the prior art de-oiling decoloration process exist can not simultaneously de-oiling and decolourize, destroy oil,
The defects of difficult is post-processed, the purpose of the present invention is that thick silkworm chrysalis oil is being extracted from silkworm chrysalis leftover bits and pieces in offer one kind, and is utilized
Thick silkworm chrysalis oil is carried out efficiently to decolourize simultaneously for modified graphite oxide and deodorization, and does not influence oil, extracts the odorless white of high-quality
The method of silkworm chrysalis oil, this method flow is short, simple to operate, cost is low, meets industrialized production.
The invention provides a kind of method that odorless white silkworm chrysalis oil is extracted in leftover bits and pieces from silkworm chrysalis, this method is by silkworm chrysalis
Leftover bits and pieces drying, after crushing, thick silkworm chrysalis oil is extracted using ultrasonic wave added organic solvent, solid-to-liquid ratio is pressed in the thick silkworm chrysalis oil of gained
0.1~0.6g:10mL adds modified graphene oxide, and 0.25~5h of adsorption treatment is carried out under 10~60 DEG C of temperature conditionss,
Filtering, obtains odorless white refined silkworm chrysalis oil；Described modified graphene oxide passes through 880~920 DEG C of high temperature by graphite powder
After processing, it is prepared using Hummers methods.
The method that odorless white silkworm chrysalis oil is extracted from silkworm chrysalis leftover bits and pieces of the present invention also includes following preferred scheme：
The solid-liquid mass volume ratio of modified graphene oxide and thick silkworm chrysalis oil is 0.2~0.5g in preferable scheme:10mL.
The temperature of adsorption treatment is 15~40 DEG C in preferable scheme.
The time of adsorption treatment is 1.8~2.5h in preferable scheme.
Modified graphite oxide, which is added in thick silkworm chrysalis oil, in preferable scheme carries out batch type, makes decoloration and deodorization more
Completely.
Graphite powder is 10~20s in the time of 880~920 DEG C of high-temperature process in preferable scheme.
Drying is that silkworm chrysalis drying is not more than into 5% to biodiversity content under the conditions of 55~65 DEG C in preferable scheme.
Granularity is crushed in preferable scheme after silkworm chrysalis drying in the range of the purpose of -40 mesh~+60.
Organic solvent is the mixed solvent of petroleum ether and hexamethylene in preferable scheme.Described petroleum ether and hexamethylene ring is excellent
Elect by volume 0.5~1.5 as:1 mixing.
Further preferred scheme：By silkworm chrysalis after drying is not more than 5% to biodiversity content under the conditions of 55~65 DEG C,
Granularity is crushed in the range of the purpose of -40 mesh~+60；It is molten using the mixing of petroleum ether and hexamethylene to crush obtained silkworm chrysalis powder
Agent carries out refluxing extraction under conditions of ultrasonic wave added, obtains thick silkworm chrysalis oil, in the thick silkworm chrysalis oil of gained by solid-to-liquid ratio 0.2~
0.5g:10mL adds modified graphene oxide, after carrying out 1.8~2.5h of adsorption treatment at a temperature of 15~40 DEG C, filtering, obtains
Odorless white refined silkworm chrysalis oil.
Optimal adsorption treatment scheme is that adsorption temp is 30 DEG C, time 2h, and modified graphene oxide is thick with silkworm chrysalis oil
The mass volume ratio of thick silkworm chrysalis oil is 0.2g:10mL.
Compared with prior art, the present invention has the advantages that：
1st, the present invention is carried out using modified graphene oxide to thick silkworm chrysalis oil first while deodorization decoloring, its percent of decolourization reach
72.45%, and good deodorization effect simultaneously, obtained refined silkworm chrysalis oil free from extraneous odour, and after thick silkworm chrysalis oil deodorization decoloring, it is modified
Graphene oxide, without influence, obtains high-quality silkworm chrysalis oil to the oil of silkworm chrysalis oil.
2nd, modified graphene oxide of the invention is carried out to thick silkworm chrysalis oil while the technique of deodorization decoloring is extremely simple, is not required to
Special equipment and reagent are wanted, modified graphene oxide need to only be added in thick silkworm chrysalis oil, places a period of time (intermittence agitation
Several times).
3rd, the present invention using modified graphene oxide makees adsorbent not only decoloration and deodorization effect is good, and is easy to and silkworm chrysalis
Oil separation, post processing are simple.
4th, the present invention is gentle using reaction condition during modified graphene oxide progress deodorization decoloring, and treatment temperature is low, when
Between it is short, oil in other compositions will not be destroyed by high-temperature oxydation.
Embodiment
Following examples are intended to further illustrate present invention, and protection scope of the present invention is not limited by the example.
The preparation of the modified graphene oxide used in the embodiment of the present invention：
2.0g graphite powders are first weighed into big porcelain boat, then porcelain boat is placed in 900 DEG C of high temperature Muffle furnace and stands 15s's
It is standby to be cooled to room temperature for taking-up after time；Next weighs 1.0g sodium nitrate into 500mL round-bottomed flasks, and adds 46mL thereto
98% concentrated sulfuric acid, the temperature of its reaction system is maintained 0 DEG C, and stir until sodium nitrate is dissolved completely in sulfuric acid solution；
Graphite powder is stirred down afterwards and is added in reaction solution, continues to stir 30min after adding；Next 6g potassium permanganate is weighed, slowly
It is added in round-bottomed flask, and stirs, after potassium permanganate all adds, continues stirring and become blackish green to reaction solution and be
Only, now round-bottomed flask is transferred to be previously set in the oil bath pan that temperature is 35 DEG C and reacts 4h under magnetic agitation, then to flask
In deionized water 92mL is slowly added dropwise, while heated to 90 DEG C, after deionization drips, continue after stirring 30min, by product
Pour into 100mL beakers, and be diluted with 124mL hot deionized waters, finally with the dioxygen water process of 60mL 3%, then by solution
Centrifuge while hot, with deionized water repeatedly washed product to neutral (pH=6.5-7).Finally by modified graphene oxide (GO)
It is put into 60 DEG C of Constant Temp. Ovens, drying for standby.
Embodiment 1
1st, extraction obtains thick silkworm chrysalis oil
First leftover bits and pieces silkworm chrysalis is dried and crushed at 60 DEG C or so, obtains water content less than 5%, granularity is -40 mesh~+60
Purpose dried silkworm chrysalis meal, organic solvent are petroleum ether and hexamethylene (1：1) mixed solution, then extracted using ultrasound-reflow method
Obtain thick silkworm chrysalis oil.
2nd, modified graphene oxide adsorbs
Take the thick silkworm chrysalis oils of 10mL, add 0.2g modified graphene oxides, 2h is then handled under the conditions of 30 DEG C, therebetween every
20min is stirred once, and reaction is taken out after terminating, and is filtered, is obtained the refined silkworm chrysalis oil of deodorization decoloring.Silkworm chrysalis oil after measure processing
Color, smell.Percent of decolourization is 71.83%, and silkworm chrysalis oil is odorless.
Embodiment 2
1st, extract the method for obtaining thick silkworm chrysalis oil and embodiment 1 is identical.
2nd, 0.2g Powdered Activated Carbons and 0.2g modified graphene oxides are separately added into the thick silkworm chrysalis oils of 10mL, in temperature 30
2h is handled under the conditions of DEG C, therebetween every 20min agitations once, reaction is taken out after terminating, and determines its percent of decolourization, as a result activated carbon
Percent of decolourization be 52.74%, have a residual odors, the percent of decolourization of modified graphene oxide is 71.83%, and odorless is remaining.
Embodiment 3
1st, extract the method for obtaining thick silkworm chrysalis oil and embodiment 1 is identical.
2nd, the thick silkworm chrysalis oils of 10mL are taken, 0.2g modified graphene oxides is added, 2h is then handled under the conditions of 30 DEG C, therebetween often
Every 20min agitations once, reaction is taken out after terminating, and is filtered, is obtained the refined silkworm chrysalis oil of deodorization decoloring.With GC measure before and after the processing
The main component of silkworm chrysalis oil, as a result as shown in table 1, as can be seen from the table, absorption is used as using modified graphene oxide (GO)
Agent has substantially no effect on silkworm chrysalis oil quality.
The main component of the silkworm chrysalis oil before and after the processing of table 1
| Title | Palmitic acid | Stearic acid | Oleic acid | Linoleic acid | Alpha-linolenic acid |
| Before processing/% | 18.4256 | 7.7675 | 36.5279 | 4.8457 | 28.5623 |
| After decolouring/% | 18.1247 | 7.8542 | 36.6250 | 4.7526 | 28.4533 |
Embodiment 4
1st, extract the method for obtaining thick silkworm chrysalis oil and embodiment 1 is identical.
2nd, temperature conditionss are changed in adsorption process, other conditions and embodiment 1 are identical, in 15~40 DEG C of temperature ranges,
Test result is as shown in table 2.
Influence of the reaction temperature of table 2 to deodorization decoloring effect
Embodiment 5
1st, extract the method for obtaining thick silkworm chrysalis oil and embodiment 1 is identical.
2nd, time conditions are changed in adsorption process, other conditions and embodiment 1 are identical.In 0.25~5h time ranges,
Test result is as shown in table 3.
Influence of the processing time of table 3 to decoloration and deodorization effect
Embodiment 6
1st, extract the method for obtaining thick silkworm chrysalis oil and embodiment 1 is identical.
2nd, modified graphene oxide dosage condition is changed in adsorption process, other conditions and embodiment 1 are identical.0.1~
In the range of 0.6g modified graphene oxides/thick silkworm chrysalis oils of 10mL, test result is as shown in table 4.
Influence of modified graphene oxide (GO) dosage of table 4 to deodorization decoloring effect
To sum up from the point of view of the experimental data of embodiment 4~6, optimum experimental condition of the invention is that adsorption temp is 30 DEG C, when
Between be 2h, the mass volume ratio of modified graphene oxide and silkworm chrysalis oil roughly silkworm chrysalis oil is 0.2g:10mL.
Claims (5)
1. the method for odorless white silkworm chrysalis oil is extracted in a kind of leftover bits and pieces from silkworm chrysalis, it is characterised in that dry silkworm chrysalis leftover bits and pieces,
After crushing, thick silkworm chrysalis oil is extracted using ultrasonic wave added organic solvent, 0.2~0.5g of solid-to-liquid ratio is pressed in the thick silkworm chrysalis oil of gained:
10mL adds modified graphene oxide, and 1.8~2.5h of adsorption treatment is carried out under 15~40 DEG C of temperature conditionss, filtering, is obtained
Odorless white refined silkworm chrysalis oil；Described modified graphene oxide by graphite powder by 880~920 DEG C of high-temperature process after, adopt
It is prepared with Hummers methods.
2. the method as described in claim 1, it is characterised in that described drying is to dry silkworm chrysalis under the conditions of 55~65 DEG C
It is not more than 5% to biodiversity content.
3. the method as described in claim 1, it is characterised in that model of the granularity in the mesh of -40 mesh~+60 is crushed to after silkworm chrysalis drying
In enclosing.
4. the method as described in claim 1, it is characterised in that described organic solvent is molten for the mixing of petroleum ether and hexamethylene
Agent.
5. the method as described in any one of Claims 1 to 4, it is characterised in that silkworm chrysalis is dried under the conditions of 55~65 DEG C and arrived
After biodiversity content is not more than 5%, granularity is crushed in the range of the purpose of -40 mesh~+60；Obtained silkworm chrysalis powder is crushed to adopt
Refluxing extraction is carried out under conditions of ultrasonic wave added with the mixed solvent of petroleum ether and hexamethylene, thick silkworm chrysalis oil is obtained, in gained
0.2~0.5g of solid-to-liquid ratio is pressed in thick silkworm chrysalis oil:10mL adds modified graphene oxide, is carried out at a temperature of 15~40 DEG C at absorption
After managing 1.8~2.5h, filtering, odorless white refined silkworm chrysalis oil is obtained.
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| CN201410447485.9A CN104250582B (en) | 2014-09-04 | 2014-09-04 | A kind of method that odorless white silkworm chrysalis oil is extracted in the leftover bits and pieces from silkworm chrysalis |
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| CN201410447485.9A CN104250582B (en) | 2014-09-04 | 2014-09-04 | A kind of method that odorless white silkworm chrysalis oil is extracted in the leftover bits and pieces from silkworm chrysalis |
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| CN101781601A (en) * | 2010-02-24 | 2010-07-21 | 陕西师范大学 | Method for extracting pupa oil from silkworm pupa by using ultrasonic wave |
| CN102965189A (en) * | 2012-11-09 | 2013-03-13 | 天津耀宇生物技术有限公司 | Method for extracting chrysalis oil |
| CN102989416A (en) * | 2012-11-30 | 2013-03-27 | 中国农业科学院油料作物研究所 | Aflatoxin adsorbent and method for removing aflatoxins in edible vegetable oil |
| CN102504958B (en) * | 2011-11-03 | 2013-10-30 | 江苏科技大学 | Method for separating unsaturated fatty acids from silkworm chrysalis oil based on composition complexation of reversible reaction |
| CN103540402A (en) * | 2013-10-31 | 2014-01-29 | 西南大学 | Method for reducing content of cholesterol in chrysalis oil |
| CN103540394A (en) * | 2013-08-27 | 2014-01-29 | 江苏科技大学 | Method for extracting silkworm pupa oil by utilizing ultrasonic assisted aqueous enzymatic method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992305A (en) * | 2012-10-25 | 2013-03-27 | 中南大学 | Graphene material and preparation method of solid graphene |
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- 2014-09-04 CN CN201410447485.9A patent/CN104250582B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781601A (en) * | 2010-02-24 | 2010-07-21 | 陕西师范大学 | Method for extracting pupa oil from silkworm pupa by using ultrasonic wave |
| CN102504958B (en) * | 2011-11-03 | 2013-10-30 | 江苏科技大学 | Method for separating unsaturated fatty acids from silkworm chrysalis oil based on composition complexation of reversible reaction |
| CN102965189A (en) * | 2012-11-09 | 2013-03-13 | 天津耀宇生物技术有限公司 | Method for extracting chrysalis oil |
| CN102989416A (en) * | 2012-11-30 | 2013-03-27 | 中国农业科学院油料作物研究所 | Aflatoxin adsorbent and method for removing aflatoxins in edible vegetable oil |
| CN103540394A (en) * | 2013-08-27 | 2014-01-29 | 江苏科技大学 | Method for extracting silkworm pupa oil by utilizing ultrasonic assisted aqueous enzymatic method |
| CN103540402A (en) * | 2013-10-31 | 2014-01-29 | 西南大学 | Method for reducing content of cholesterol in chrysalis oil |
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